CN106629696A - Preparation of reduced graphene oxide thin film by virtue of vacuum evaporation method - Google Patents
Preparation of reduced graphene oxide thin film by virtue of vacuum evaporation method Download PDFInfo
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- CN106629696A CN106629696A CN201610835913.4A CN201610835913A CN106629696A CN 106629696 A CN106629696 A CN 106629696A CN 201610835913 A CN201610835913 A CN 201610835913A CN 106629696 A CN106629696 A CN 106629696A
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Abstract
The invention discloses a novel process for preparing a reduced graphene oxide thin film. The process is characterized in that a graphene oxide thin film is prepared by adopting a graphene oxide solution through a stick coating method and is reduced to obtain the reduced graphene oxide thin film by a method of vacuum-evaporating an aluminum film. The process mainly comprises the following steps: (1) preparing the graphene oxide solution from flake graphite by virtue of an improved Hummers method; (2) coating a PET substrate with the graphene oxide solution to prepare the graphene oxide thin film by virtue of the stick coating method; (3) evaporating the aluminum film with a certain thickness on the graphene oxide thin film by adopting a vacuum evaporation process; (4) placing the sample in a hydrochloric acid solution for impregnation, flushing the sample with a diluted hydrochloric acid and de-ionized water, and performing drying to obtain the reduced graphene oxide thin film. According to the process, a large-area reduced graphene oxide thin film can be efficiently and environment-friendlily prepared with low cost.
Description
Technical field
The invention belongs to the synthetically prepared technical field of carbon nanomaterial, is related to a kind of redox graphene of novelty thin
The preparation technology of film.
Background technology
Graphene is a kind of new two-dimensional nano crystalline material, with excellent electric property, mechanical property, calorifics
Energy and optical property.These excellent performances allow Graphene to send out in transparent conductive film, flexible electronic device, field
Penetrate, the aspect tool such as transistor, hydrogen storage, ultracapacitor and sensor has broad application prospects.But how economical and effective
Acquisition large-size graphene film be an outstanding problem.In the last few years, graphene oxide was considered as that to obtain Graphene thin
The most important presoma of film, currently prepares the method for graphene oxide generally using Hummers methods or improved Hummers methods.
This method is simple, easy to operate, with low cost, and graphene oxide solution is easy to form film in any substrate, and oxygen is prepared at present
The method that the method for graphite alkene film has spraying process, spin-coating method, stick coating method and self-assembly method, wherein, stick coating method has been found to can
To prepare large-area oxidation graphene film.Because graphene oxide is insulation, therefore it is to prepare conductive stone to reduce
The topmost process of black alkene film.Method of reducing includes thermal reduction and electronation, and requirement of the thermal reduction to substrate is higher, no
Beneficial to the preparation of fexible film, the reducing agent of electronation is typically all strong reductant, toxic and be easily destroyed graphite oxide
The surface topography of alkene film, so needing to seek a kind of low cost, quick and nondestructive method of reducing.Aluminium is in acid medium
Graphene oxide film can be reduced by electro transfer down, so taking a kind of method reduction-oxidation of vacuum evaporation aluminium film
Graphene film, such that it is able to rapidly, without devastatingly obtaining the redox graphene with large-area electrically conducting transparent
Film.
The content of the invention
It is an object of the invention to provide a kind of preparation method of novel oxidation graphene film.
Technical scheme is as follows：First graphene oxide solution is prepared by improved Hummers methods；So
Afterwards graphene oxide film is prepared with stick coating method, certain thickness aluminium film is deposited with by the method for vacuum evaporated aluminium.Finally by sample
Product are put in hydrochloric acid solution and soak, and after watery hydrochloric acid and deionized water rinsing post-drying oxidation graphene film is obtained.
The main innovation point of the present invention is as follows：Large-area graphene oxide film can be prepared using stick coating method, then led to
Cross the method for vacuum evaporation aluminium film and redox graphene prepares oxidation graphene film in hydrochloric acid solution, it is right
, without destructiveness, film surface is smooth, and roughness is low for graphene membrane surface.The invention provides a kind of novel, quick, environmental protection,
The method of low cost is preparing oxidation graphene film.
The method that graphene oxide film is prepared in the inventive method is as follows：With crystalline flake graphite as raw material, using improved
Hummers methods prepare graphene oxide, prepare graphene oxide solution, and stick coating method prepares graphene oxide film, by control
The diameter and solution concentration of rod, can obtain the graphene oxide film of different-thickness.
The reduction process of graphene oxide film is as follows in the inventive method：In graphene oxide film surface vacuum evaporation
Thickness is the aluminium film of 1-50nm, is put in the hydrochloric acid solution of 1-12M and soaks, with watery hydrochloric acid and deionized water rinsing post-drying, i.e.,
Oxidation graphene film is obtained.
The present invention has found when oxidation graphene film is prepared, when graphene oxide film is prepared, when vacuum is steamed
When the aluminium film thickness of plating and the ratio of graphene oxide thickness are less than 1.5 times, it is not thorough enough that graphene oxide film is reduced；Work as aluminium
When film thickness increases, graphene oxide is reduced completely, the electric conductivity of the oxidation graphene film obtained after final reduction
Can be more preferably；When concentration of hydrochloric acid is 10M, the electric conductivity of the oxidation graphene film obtained after final reduction is more preferable.
Reagent and material used by the present invention：Crystalline flake graphite, PET film, vacuum deposition apparatus, aluminum shot, concentrated hydrochloric acid are
Analysis is pure.
Description of the drawings
Fig. 1 is the preparation technology schematic diagram of oxidation graphene film.
Fig. 2 is the relation between oxidation graphene film surface resistance and light transmittance.
Specific embodiment
The present invention is elaborated with reference to instantiation.
With 32 mesh crystalline graphite powders as raw material, using Hummers methods are improved graphene oxide solution is prepared.Configuration is not
With the graphene oxide solution of concentration, the graphene oxide film for obtaining that thickness is 10nm is applied by rod, in vacuum evaporation case
Evaporation thickness is the aluminium film of 15nm, soaks 5min in the hydrochloric acid solution of 10M, then with after watery hydrochloric acid and deionized water rinsing for several times
Post-drying, you can obtain oxidation graphene film.
Claims (9)
1. a kind of preparation technology of novel oxidation graphene film, it is characterised in that passed through using graphene oxide solution
Stick coating method prepares graphene oxide film, and by the method reduction of vacuum evaporation aluminium film oxidation graphene film is obtained, and
And large area, low cost, efficient, environmental protection.Preparation process is as follows：Raw material is made with graphite oxygen is prepared by improved Hummers methods
Graphite alkene solution, by stick coating method graphene oxide film is prepared, by vacuum evaporated aluminium, on graphene oxide film surface
The aluminium film of evaporation different-thickness, is reduced in hydrochloric acid solution, then is gone back with watery hydrochloric acid and deionized water rinsing post-drying
Former graphene oxide film.
2. method according to claim 1, it is characterised in that the graphene oxide sheet footpath size for obtaining concentrates on 10-20 μm
In the range of.
3. method according to claim 1, it is characterised in that the concentration of graphene oxide solution is 1-10mg/ml, rod is applied
A diameter of 0.2-0.8cm of Meyer rod used by method.
4. method according to claim 1, it is characterised in that the speed of vacuum evaporation is
5. method according to claim 1, it is characterised in that the aluminium film thickness of vacuum evaporation is 1-50nm.
6. method according to claim 1, it is characterised in that the concentration of hydrochloric acid used is 1-12M.
7. method according to claim 1, it is characterised in that the reduction reaction time needs 2-20 minutes.
8. method according to claim 1, it is characterised in that the surface resistance scope of the oxidation graphene film for obtaining
For 0.1-25k Ω/sq, range of transmittance is 60-95%.
9. method according to claim 1, it is characterised in that surface roughness declines and film surface is not destroyed after reduction.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610835913.4A CN106629696A (en) | 2016-09-20 | 2016-09-20 | Preparation of reduced graphene oxide thin film by virtue of vacuum evaporation method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201610835913.4A CN106629696A (en) | 2016-09-20 | 2016-09-20 | Preparation of reduced graphene oxide thin film by virtue of vacuum evaporation method |
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| CN106629696A true CN106629696A (en) | 2017-05-10 |
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| CN201610835913.4A Pending CN106629696A (en) | 2016-09-20 | 2016-09-20 | Preparation of reduced graphene oxide thin film by virtue of vacuum evaporation method |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108996496A (en) * | 2018-07-23 | 2018-12-14 | 哈尔滨工业大学 | A method of preparing graphene/graphene mixed film |
| CN115246949A (en) * | 2021-04-27 | 2022-10-28 | 天津工业大学 | Reduced graphene oxide flexible conductive film and three-step moderate reduction preparation process thereof |
Citations (3)
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| WO2009049375A1 (en) * | 2007-10-19 | 2009-04-23 | University Of Wollongong | Process for the preparation of graphene |
| CN102557013A (en) * | 2010-12-28 | 2012-07-11 | 国家纳米科学中心 | Preparation method for reduced graphene oxide |
| CN103043654A (en) * | 2011-10-12 | 2013-04-17 | 国家纳米科学中心 | Film containing graphene and/or graphene oxide, and preparation method thereof |
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2016
- 2016-09-20 CN CN201610835913.4A patent/CN106629696A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2009049375A1 (en) * | 2007-10-19 | 2009-04-23 | University Of Wollongong | Process for the preparation of graphene |
| CN102557013A (en) * | 2010-12-28 | 2012-07-11 | 国家纳米科学中心 | Preparation method for reduced graphene oxide |
| CN103043654A (en) * | 2011-10-12 | 2013-04-17 | 国家纳米科学中心 | Film containing graphene and/or graphene oxide, and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| ZHUANG-JUN FAN ET AL.: "Facile Synthesis of Graphene Nanosheets via Fe Reduction of Exfoliated Graphite Oxide", 《ACS NANO》 * |
| 黄守伦主编: "《实用化学热处理与表面强化新技术》", 30 June 2002, 机械工业出版社 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108996496A (en) * | 2018-07-23 | 2018-12-14 | 哈尔滨工业大学 | A method of preparing graphene/graphene mixed film |
| CN115246949A (en) * | 2021-04-27 | 2022-10-28 | 天津工业大学 | Reduced graphene oxide flexible conductive film and three-step moderate reduction preparation process thereof |
| CN115246949B (en) * | 2021-04-27 | 2023-11-03 | 天津工业大学 | Reduced graphene oxide flexible conductive film and three-step moderate reduction preparation process thereof |
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